CN101962447B - Compound talcpowder and preparation method thereof - Google Patents
Compound talcpowder and preparation method thereof Download PDFInfo
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- CN101962447B CN101962447B CN 200910108966 CN200910108966A CN101962447B CN 101962447 B CN101962447 B CN 101962447B CN 200910108966 CN200910108966 CN 200910108966 CN 200910108966 A CN200910108966 A CN 200910108966A CN 101962447 B CN101962447 B CN 101962447B
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Abstract
The invention provides compound talcpowder and a preparation method thereof. The compound talcpowder comprises talcpowder, titanate and silane; the compound talcpowder has a diameter range of between 100 nm and 3 um and the average particle size of between 350 and 400 nm; and based on the total volume of the talcpowder, particles with the diameter of between 100 and 500 nm account for 68 to 73 percent, particles with the diameter of between 0.5 and 1.0 um account for 20 to 24 percent, and particles with the diameter of between 1 and 3 um account for 7 to 8 percent. The compound talcpowder prepared by the method provided by the invention has the characteristics of good uniformity of particle size distribution and the maximum particle size of less than 3 mu m.
Description
Technical field
The present invention relates to a kind of composite talc powder and preparation method thereof.
Background technology
Talcum is the moisture magnesium silicate of a kind of stratiform, have good electrical insulation capability, thermotolerance, mechanical property, it joins hot expansibility and the mechanical property that can improve matrix material in the middle of the organic materials as stopping composition, talcum and strong acid and highly basic are generally all inoperative, have good chemical stability; China's talcum deposit is abundant, and cheap, its many characteristics have determined that it is widely used in fields such as electronic package material, military wrapping material, automobile instruments as stopping composition.Along with above-mentioned field to meticulous microminiaturized the improving constantly of requiring of product, its to the size of stopping composition and and organic resin between consistency higher demand has been proposed.
Present domestic superfine talcum powder factory, median size generally can reach 2-5um, as producing median size in the prior art at 1 to 2um talcum powder, but exist particle size distribution inhomogeneous, larger particle diameter can reach 10 to 25um, can't guarantee the homogeneity of product, these fillers bigger than normal join the performance that can have a strong impact on product in the middle of the organic materials, can't satisfy the requirement of the electron trades such as PCB.In the fine electronic industry, consider that the size control of dosing material is in 5% to 20% of its product size on the one hand, consider that on the other hand the adding of dosing material can not make it produce sedimentation in the middle of resin, be that the pedesis effect is better than action of gravity, and oarse-grained existence can cause the generation of above-mentioned phenomenon.Consider, talcous maximum particle diameter must not require above 3um.
Talcum powder is sheet structure, when its most of particle diameter is larger, be easier to its pulverizing under the high speed shear power effect by grinding medium, but when pulverized packing material size diminishes, reuniting strengthens, and its intergranular space diminishes, and mill efficiency is reduced, even lengthen working hours, the part particle diameter does not reach enough little yet.All will at high temperature carry out talcous surface modification treatment at present in addition, this has also affected and has ground diminishing of packing material size.In order to reach absolute ultra-fine requirement, a lot of producers update the preparation technology of extra fine talc powder, disclose the method that a kind of wet method prepares talc powder body such as the prior art Patent, and the method comprises:
1) raw material is carried out fragmentation
2) material after the fragmentation is carried out grinding;
3) material behind the grinding is carried out slurrying
4) material behind the grinding is carried out the stripping of wet type Ultrafine Grinding;
5) material after the Ultrafine Grinding stripping is carried out strong drying and collects goods.
Prepare superfine talcum powder by above-mentioned method, but the method can't satisfy the absolute particle size of particle at 2-3um, and particle size distribution range is wide, the homogeneity of product is bad, and relatively poor with organic consistency.
Summary of the invention
It is little that technical problem to be solved by this invention provides a kind of particle diameter, the size distribution homogeneous, composite talc powder.
The invention provides a kind of composite talc powder, comprise talcum powder, titanic acid ester, silane, this talcous diameter range is 100nm～3um, median size is 350～400nm, take the cumulative volume of composite talc powder as benchmark, wherein 100～500nm accounts for 68～73%, and 0.5～1.0um accounts for 20～24%, and 1～3um accounts for 7%～8%.
The present invention also provides a kind of method for preparing composite talc powder, and the method comprises:
1) take by weighing in proportion talcum powder, ethanol, put into shredder, carry out the first time and grind, then add the partial-titanium acid esters, carry out second time and grind, the titanic acid ester of adding remainder in the shredder is ground for the third time again, obtains first ground slurry;
2) grind for the 4th time carrying out after the first ground slurry for preparing in the step (1) and the silane mixture that takes by weighing, obtain ground slurry, with this ground slurry oven dry, acquisition composite talc powder.This composite talc powder, comprise talcum powder, titanic acid ester, silane, the diameter range of this composite talc powder is 100nm～3um, median size is 350～400nm, take the cumulative volume of composite talc powder as benchmark, wherein 100～500nm accounts for 68～73%, and 0.5～1.0um accounts for 20～24%, and 1～3um accounts for 7%～8%.
Preparing composite talc powder by method provided by the invention, not only to have a particle diameter little, the particle diameter distribution homogeneous, and have the advantage good with the organic resin consistency.
Embodiment
A kind of composite talc powder is provided among the present invention, this talcum powder comprises talcum powder, titanic acid ester, silane, the diameter range of this composite talc powder is 100nm～3um, median size is 350～400nm, take the cumulative volume of composite talc powder as benchmark, wherein 100～500nm accounts for 68～73%, and 0.5～1.0um accounts for 20～24%, and 1～3um accounts for 7%～8%.
Take the composite talc powder gross weight as benchmark, talcum powder accounts for that 86～99wt%, titanic acid ester account for 0.5～10wt%, silane accounts for 0.5～5wt%.
In the preferred case take the composite talc powder gross weight as benchmark, talcum powder accounts for that 94～98wt%, titanic acid ester account for 1～4wt%, silane accounts for 1～2wt%.
Wherein, described titanic acid ester is the titanic acid ester with following structure:
(RO)
N-Ti-(OX-R`-Y)
M
Wherein, R is the carbochain alkyl of C2-C5, and R` is the carbochain alkyl of 6≤C≤30, and X is C, N, P, S element, and Y is amino, epoxy group(ing), and N is the arbitrary value of 1≤N≤4, and N+M≤6.
Have between titanic acid ester and talcum powder main component SiO-, the MgO-and adsorb preferably bonding action, wherein better with single alcoxyl tetra-sodium type effect, its water tolerance is better, and non-coupling side molecular structure volume steric hindrance is large, more is conducive to both couplings.Titanic acid ester is selected from one or more in sec.-propyl three oleoyl titanic acid ester, sec.-propyl three (dioctylphyrophosphoric acid ester acyl group) titanic acid ester, sec.-propyl three (dioctyl phosphoric acid ester acyl group) titanic acid ester, sec.-propyl three (N-ethylamino-ethylamino) titanic acid ester etc. under the preferable case; titanate coupling agent also plays the effect of grinding aid in process of lapping simultaneously, and the effect of grinding is played larger impact.Used titanic acid ester can be by commercially available, such as the superior NDZ101 of great company and the NDZ201 of Nanjing Dawning of advocating among the present invention.
Used silane is one or more that have in the silane of following structure among the present invention:
RSiX
3
Wherein, R has avidity or response capacity and is the active function groups of low molecular chain with polymer molecule, and is a kind of such as amino, epoxy group(ing), amido, aminopropyl, and X is a kind of in halogen, alkoxyl group, the acyloxy.
Along with grinding diminishing of particle diameter, the non-coupling group volume of titanic acid ester is larger, so that produced white space (not coupling zone) by levigate talcum powder surface, it not only can increase the reunion of filler, hinder the refinement of abrasive grains, also can arrive the consistency that has influence between itself and the organic polymer.The used silane of the present invention not only will have good coupled action with filler, also needs the characteristics that have volume little, simple in structure, such as the non-coupling pendant groups small molecule structure that is straight chain.Silane is selected from γ aminopropyltriethoxy silane, γ-(2 in the preferred case, 3 glycidoxies) propyl trimethoxy silicane, γ-r-chloropropyl trimethoxyl silane, in the rare ethyl triethoxy silicane alkane of second etc. one or more, adopt silane coupling agent as another grinding aid among the present invention, because the adding of silane coupling agent is so that the further refinement of the particle of composite talc powder.Used silane can be by commercially available, such as the superior KH550 of great company and the A-1100 of Dow Corning Corporation of advocating among the present invention.
Wherein, mainly be as main take the titanate coupling agent class among coupling agent the present invention, such as NDZ201, the contriver finds that by lot of experiments not only there is good chemical coupling ability on itself and talcum powder surface, also because the impact of its sterically hindered structure, reduce crosslinked between the coupling agent, improved itself and large particle diameter talcum powder surface bond ability, thereby promoted the dispersion efficiency of system.Along with the carrying out of circular grinding, properties-correcting agent adds with batch mode, and large particle diameter talcum powder is constantly by refinement in the system, and its surface also constantly produces the new spacing zone, and again with the properties-correcting agent coupling, again refinement, constantly circulation is to reach best mill efficiency; When the talcum powder granularity drops to a certain degree, this properties-correcting agent is not remarkable for the help of grinding, for further refinement powder, improve mill efficiency, need to add a kind of silane coupling agent, its structure is that an end can have good coupling capacity with the talcum powder surface, and the other end can have with organic polymer the group of excellent compatibility, group that the more important thing is itself and powder surface bonding will be take the small molecules straight chain as main, such as KH550.It joins in the circular grinding system, because the before impact of the sterically hindered structure of properties-correcting agent, powder surface is residual white space, namely not by the coupling zone, cause further refinement talcum powder Efficiency Decreasing, and the adding of this small molecules straight chain coupling agent makes these white spaces also by good bonding, improve mill efficiency, thereby obtain the particle absolute diameter all less than 3um, and have the talcum powder with the resin excellent compatibility.
The present invention also provides a kind of preparation method of composite talc powder, comprising:
1) takes by weighing in proportion talcum powder, ethanol, titanic acid ester and put into shredder, carry out the first time and grind, then add the partial-titanium acid esters, carrying out the second time grinds, add again the titanic acid ester of remainder behind the certain hour in the shredder, grind for the third time, obtain first ground slurry;
2) grind for the 4th time carrying out after the first ground slurry for preparing in the step (1) and the silane mixture that takes by weighing, obtain ground slurry, with this ground slurry oven dry, obtain composite talc powder, described composite talc powder, comprise talcum powder, titanic acid ester, silane, it is characterized in that, this talcous diameter range is 100nm～3um, median size is 350～400nm, and take the cumulative volume of composite talc powder as benchmark, wherein the particle of 100～500nm accounts for 68～73%, 0.5 the particle of～1.0um accounts for 20～24%, 1～3um particle accounts for 7%～8%.
Be 0.1～1.0 according to weight ratio first in step 1: 1.0～1.0 take by weighing talcum powder, ethanol, then mixture is added in the shredder, carrying out the first time grinds, wherein used talcous average particulate diameter is that 500-5000 can be by talcum powder commercially available as bright and beautiful Long Hui company 2500 order models, when grinding for the first time, operational condition is shredder rotating speed 1000～1500rpm, through after the grinding of 3h time, the titanic acid ester of 0.25～5wt% is added wherein, carrying out the second time under the condition of 1500～1800rpm grinds, grinding through the 3h time, the titanic acid ester that again adds 0.25～5wt%, the reason that titanic acid ester adds in batches is owing to the carrying out along with circular grinding, large particle diameter talcum powder is constantly by refinement in the system, its surface produces the new spacing zone simultaneously, thereby this moment again add titanic acid ester further with the talcum powder coupling, grind again refinement, to reach best mill efficiency, the condition of grinding for the third time is 1500～1800rpm, pass through again the grinding of 3h time, the silane coupling agent that adds 0.5～5wt%, the condition of grinding for the 4th time is 1500～1800rpm, grind the ground slurry finally obtain composite talc powder through four times, this slurry is put into vacuum drying oven under 60～120 degrees centigrade condition, dry and namely get composite talc powder provided by the invention.
The effect that wherein adds ethanol in first time process of lapping is the dispersion medium as grinding system, and talcum powder has good dispersiveness in ethanol, be conducive to grind, and be cheap solvent and recyclable recycling from considering economically it.
Grind by four times among the present invention, finally obtain composite talc powder, the condition of wherein grinding for four times is as follows:
The condition of grinding for the first time is shredder rotating speed: 1000～1500rpm, time 3～9h;
The condition of grinding for the second time is shredder rotating speed: 1500～1800rpm, time 3～6h;
The condition of grinding for the third time is shredder rotating speed: 1500～1800rpm, time 3-4h;
The condition of grinding for the 4th time is shredder rotating speed: 1500～1800rpm, time 3-4h.
Repeatedly grind through four times, and in different grinding steps, add different types of coupling agent so that the grain diameter of final composite talc powder less than 3 microns.
In step 1 talcum powder of using be commercially available particle diameter at 1000-5000 purpose talcum powder, the 2500 order talcum powder of producing such as bright and beautiful Long Hui company.
The weight ratio of talcum powder, titanic acid ester, silane is 86～99: 0.5～10 in the composite talc powder process of preparation: 0.5～5.
The below further specifies composite talc powder provided by the present invention and preparation method thereof with concrete embodiment.
Embodiment 1
Present embodiment is used for illustrating composite talc powder provided by the present invention and preparation method thereof.
Taking by weighing median size is the talcum powder 10Kg that 2500 orders brocade Long Hui company produces; ethanol 20Kg; put into shredder (Qingdao joins the auspicious precision optical machinery DMQ of company limited series); mix under the condition that is incorporated in 1000rpm and grind 3h; sec.-propyl three (the dioctylphyrophosphoric acid ester acyl group) titanate coupling agent (being called for short NDZ201) of 100g is added wherein; under the condition of 1200rpm, grind 3h; the NDZ201 of 100g is added in the above-mentioned mixture; under 1500 condition, grind 3h; obtain ground slurry; under the condition of 1800rpm, grind 3h to the γ aminopropyltriethoxy silane coupling agent that obtains to add in the ground slurry 100g (being called for short KH550) again; obtain ground slurry, this ground slurry is put into vacuum drying oven under 60～120 ℃ of conditions, dry and to obtain composite talc powder sample T1.
Embodiment 2
Present embodiment is used for illustrating composite talc powder provided by the present invention and preparation method thereof.
Taking by weighing median size is the talcum powder 20Kg of the imperial brightness of 1000 purposes brocade; ethanol 20Kg; put into shredder (Qingdao joins the auspicious precision optical machinery DMQ of company limited series); mix under the condition that is incorporated in 1000rpm and grind 5h; sec.-propyl three (the dioctylphyrophosphoric acid ester acyl group) titanate coupling agent (being called for short NDZ201) of 400g is added wherein; under the condition of 1200rpm, grind 4h; the NDZ201 of 200g is added in the above-mentioned mixture; under 1500 condition, grind 3h; obtain ground slurry; under the condition of 1800rpm, grind 3h to the γ aminopropyltriethoxy silane coupling agent that obtains to add in the ground slurry 200g (being called for short KH550) again; obtain ground slurry, this ground slurry is put into vacuum drying oven under 60～120 ℃ of conditions, dry and to obtain composite talc powder sample T2.
Embodiment 3
Present embodiment is used for illustrating composite talc powder provided by the present invention and preparation method thereof.
Taking by weighing median size is the talcum powder 10Kg that the safe company limited in 2000 purpose skies produces; ethanol 10Kg; put into shredder (Qingdao joins the auspicious precision optical machinery DMQ of company limited); mix under the condition that is incorporated in 1000rpm and grind 4h; sec.-propyl three (the dioctylphyrophosphoric acid ester acyl group) titanate coupling agent (being called for short NDZ201) of 100g is added wherein; under the condition of 1200rpm, grind 3h; the NDZ201 of 200g is added in the above-mentioned mixture; under 1500 condition, grind 3h; obtain ground slurry; under the condition of 1800rpm, grind 3h to the γ aminopropyltriethoxy silane coupling agent (KH550) that obtains adding 200g in the ground slurry again; obtain ground slurry, this ground slurry is put into vacuum drying oven under 60～120 ℃ of conditions, dry and to obtain composite talc powder sample T3.
Comparative Examples 1
This Comparative Examples prepares sample CT1 according to the method for recording and narrating among the patent CN 1203124A.
Embodiment 4-6
Present embodiment is used for the size distribution test of the prepared sample T1-T3 of test implementation example 1-3, and test result sees Table 1.
The size distribution test
Sample is put into instrument: particle-size analyzer (MICROTRAC S3500), carry out the sreen analysis test.Test result is seen table 1 in the Figure of description.
Comparative Examples 2
This Comparative Examples is used for the properties of test comparison example 1 prepared sample CT1, and the sreen analysis performance test of wherein putting down in writing among granularity performance test and the embodiment 4-6 is identical, and test result sees Table 1.
Table 1
| 100～500 nanometers account for percent by volume | 500～1000 nanometers account for percent by volume | The 1-3 micron accounts for percent by volume | Account for percent by volume greater than 3 microns | |
| Embodiment 1 | 68.15％ | 23.96％ | 7.89％ | 0％ |
| Embodiment 2 | 72.88％ | 20.12％ | 7.00％ | 0％ |
| Embodiment 3 | 70.73％ | 21.65％ | 7.62％ | 0％ |
| Comparative Examples 1 | 50.23％ | 30.66％ | 15.29％ | 3.82％ |
As can be seen from Table 1, the size distribution of the sample T2 that embodiment 2 prepares among the present invention is that the particle of 100～500 nanometers accounts for percent by volume 72.88%, it is 23.96% that the particle of 500～1000 nanometers accounts for percent by volume, the particle of 1-3 micron accounts for percent by volume 7.00%, account for percent by volume 0% greater than 3 microns, and the size distribution of sample CT1 of preparation is that the particle of 100～500 nanometers accounts for percent by volume 50.23% in the Comparative Examples 1, the particle of 500～1000 nanometers accounts for percent by volume 30.66%, the particle of 1-3 micron accounts for percent by volume 15.29%, account for percent by volume 3.82% greater than 3 microns particles, find out by contrast, the particle major part of sample provided by the present invention is distributed in the scope of 100～500 nanometers, the homogeneous better performances of product is described, and the maximum particle diameter that also shows sample provided by the present invention in the table 1 does not have above 3 microns, and in the Comparative Examples 1 among the prepared sample CT1 particle greater than 3 microns account for percent by volume 3.82%, the particle diameter of the particle of visible sample provided by the present invention is less than the grain diameter of CT1.
Claims (9)
1. composite talc powder, comprise talcum powder, titanic acid ester, silane, it is characterized in that, the particle size range of this composite talc powder is 100nm～3 μ m, median size is 350～400nm, and take the cumulative volume of composite talc powder as benchmark, size distribution is that the particle of 100～500nm accounts for 68～73%, 0.5 the particle of～1.0 μ m accounts for 20～24%, the particle of 1～3 μ m accounts for 7%～8%.
2. talcum powder according to claim 1, wherein, take the composite talc powder gross weight as benchmark, talcum powder accounts for that 86～99wt%, titanic acid ester account for 0.5～10wt%, silane accounts for 0.5～5wt%.
3. talcum powder according to claim 2, wherein, take the composite talc powder gross weight as benchmark, talcum powder accounts for that 94～98wt%, titanic acid ester account for 1～4wt%, silane accounts for 1～2wt%.
4. composite talc powder according to claim 1, wherein said titanic acid ester is selected from one or more in sec.-propyl three oleoyl titanic acid ester, sec.-propyl three (dioctylphyrophosphoric acid ester acyl group) titanic acid ester, sec.-propyl three (dioctyl phosphoric acid ester acyl group) titanic acid ester, sec.-propyl three (N-ethylamino-ethylamino) titanic acid ester.
5. composite talc powder according to claim 1, wherein said silane are one or more that have in the silane of following structure:
RSiX
3
Wherein, R is a kind of in amino, epoxy group(ing), amido, the aminopropyl, and X is a kind of in halogens, alkoxyl group, the acyloxy.
6. composite talc powder according to claim 5, wherein said silane is γ aminopropyltriethoxy silane.
7. the preparation method of a composite talc powder comprises:
1) takes by weighing in proportion talcum powder, ethanol, titanic acid ester, first talcum powder and ethanol are put into shredder, carry out the first time and grind, then add the partial-titanium acid esters, carry out the second time and grind, add again the titanic acid ester of remainder in the shredder, grind for the third time, obtain first ground slurry;
2) take by weighing in proportion first ground slurry and the silane for preparing in the step (1), carrying out the 4th time after the mixing grinds, obtain ground slurry, with this ground slurry oven dry, obtain composite talc powder, described composite talc powder, comprise talcum powder, titanic acid ester, silane, it is characterized in that this talcous diameter range is 100nm-3 μ m, median size is 350～400nm, take the cumulative volume of composite talc powder as benchmark, wherein 100～500nm accounts for 68～73%, and 0.5～1.0 μ m accounts for 20～24%, and 1～3 μ m accounts for 7%～8%.
8. the preparation method of the composite talc powder described in according to claim 7, the weight ratio of wherein said talcum powder, ethanol is 0.1～1.0: 1.0～1.0.
9. the preparation method of composite talc powder according to claim 7, the weight ratio of wherein said talcum powder, titanic acid ester, silane is 86～99: 0.5～10: 0.5～5.
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| CN104231317A (en) * | 2014-08-21 | 2014-12-24 | 安徽吉安特种线缆制造有限公司 | Modified talcum for anti-aging chlorinated polyethylene cable material and preparation method thereof |
| CN109054178A (en) * | 2018-07-20 | 2018-12-21 | 吴伟华 | A kind of talcum powder and preparation method thereof improving toughness |
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| US4604421A (en) * | 1984-03-27 | 1986-08-05 | Sumitomo Chemical Company, Limited | Polypropylene resin composition comprising talc having specified average diameter and particle size |
| CN1765741A (en) * | 2004-10-29 | 2006-05-03 | 中南大学 | Method for preparing micro/mesoporous material using talc |
| CN101230210A (en) * | 2007-12-28 | 2008-07-30 | 河北工业大学 | Method for preparing organic modified silicate mineral clay |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4604421A (en) * | 1984-03-27 | 1986-08-05 | Sumitomo Chemical Company, Limited | Polypropylene resin composition comprising talc having specified average diameter and particle size |
| CN1765741A (en) * | 2004-10-29 | 2006-05-03 | 中南大学 | Method for preparing micro/mesoporous material using talc |
| CN101230210A (en) * | 2007-12-28 | 2008-07-30 | 河北工业大学 | Method for preparing organic modified silicate mineral clay |
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| Title |
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| 杨华明等.矿物表面机械化学改性新工艺研究.《金属矿山》.2000,(第7期),第13-16,28页. * |
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